CN105254340A - Method for producing calcium superphosphate and calcium superphosphate compound fertilizer - Google Patents
Method for producing calcium superphosphate and calcium superphosphate compound fertilizer Download PDFInfo
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- CN105254340A CN105254340A CN201510877123.8A CN201510877123A CN105254340A CN 105254340 A CN105254340 A CN 105254340A CN 201510877123 A CN201510877123 A CN 201510877123A CN 105254340 A CN105254340 A CN 105254340A
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- China
- Prior art keywords
- calcium superphosphate
- sulfuric acid
- phosphorus ore
- grinding
- fertilizer
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Abstract
The invention discloses a method for producing calcium superphosphate and calcium superphosphate compound fertilizer and belongs to the field of agricultural fertilizer. According to the method, concentrated sulfuric acid and phosphorite are mixed under mechanical agitation grinding force, preparation of calcium superphosphate, neutralizing pretreatment and preparation of compound fertilizer are combined organically, calcium superphosphate compound fertilizer is prepared directly, complicated technological processes are avoided, production efficiency is improved, and production cost is reduced.
Description
Technical field
The present invention relates to genus field of agricultural fertilizer, relate to a kind of method of producing calcium superphosphate and Chemical Mixed Fertilizer thereof more specifically.
Background technology
Calcium superphosphate main component is monocalcium phosphate Ca (H
2pO
4)
2with gypsum CaSO
42H
2o, containing effective P
2o
514% ~ 20%, wherein 80% ~ 95% is water-soluble, belongs to water soluble quick-acting phosphate fertilizer, simultaneously containing moderate-elements such as the Calcium Magnesium Sulphurs required for crop, directly can make phosphate fertilizer, also can be used for compound fertilizer making.
The production of current calcium superphosphate mainly adopts diluted acid breeze method and concentrated acid pulp process two kinds of techniques.Diluted acid breeze method is mixed in mixing tank with certain density dilute sulphuric acid by the phosphorus ore of drying in advance, pulverizing, and then through changing into, slaking, the operation such as cutting obtain calcium superphosphate; Concentrated acid ore pulp rule the phosphorus ore of raw ore and undried, pulverization process is added ball milling in ball mill together with water prepare ore pulp, then measures through gauger with 98% vitriol oil and drop into the operations such as mixing tank carries out mixing, changes into, slaking, cutting and obtain calcium superphosphate.The principal reaction that sulfuric acid decomposition phosphorus ore manufactures calcium superphosphate is:
2Ca
5F(PO
4)
3+7H
2SO
4+3H
2O=3Ca(H
2PO
4)
2·H
2O+7CaSO
4+2HF
Real reaction carries out in two stages: the first stage is that sulfuric acid and part phosphorus ore react and generate phosphoric acid and calcium sulfate, and this single step reaction is very fast, can complete in several minutes; Subordinate phase is that phosphoric acid and another part phosphorus ore generated reacts and generate monocalcium phosphate, and this single step reaction controls by Liquid Phase Diffusion, and speed very slowly, continue several days or a few weeks.Diluted acid breeze method and concentrated acid pulp process two kinds of techniques all need to introduce moisture in reactive system.When the moisture bringing reactive system into is more, then sluggish, generates liquid phase too much, generates phosphoric acid concentration and serves diluting effect, slow down the speed of response of subordinate phase, be unfavorable for Ca (H the first stage
2pO
4)
2h
2the generation of O and crystallization, extend the curing time.Especially because the ore pulp critical flow moisture (namely can make the minimum ore pulp water content needed for ore pulp flowing during phosphorus ore wet ball grinding) of domestic most phosphorus ore is higher than mass fraction 28%, have even up to mass fraction 40%, add the too much water yield when employing concentrated acid pulp process technique forces during ball milling, thus cause too high be above standard (≤14%) of calcium superphosphate product moisture; Reduce moisture, sulfuric acid concentration is then made to improve, reaction process effect is fierce, reaction system heat release, and temperature raises, moisture evaporation is more, amount of liquid phase is less, the speed of response of subordinate phase is accelerated, because this reducing the water content of calcium superphosphate, improve the physical properties of product, improve the content of available phosphorus.But concentration and temperature are too high, the speed that the first stage can be made to react is too fast, and the calcium sulfate tiny crystals of generation is deposited on the surface of ground phosphate rock, forms the calcium sulfate wrap film of one deck densification, hinder sulfuric acid and phosphoric acid to ground phosphate rock internal divergence, also make subordinate phase react and carry out slowly.
Binary or triple super(phosphate) series compound fertilizer production technology extensively adopt granulating method.Base fertilizer by powdery, certain fineness mixes; as using urea as nitrogenous source, calcium superphosphate is as main phosphorus source, Repone K or potassium sulfate as potassium source; at binding agent as under the effect of water, acid; in the granulating equipment of the kind such as disk or cylinder after granulation, through the large series products that the operations such as super-dry, screening, cooling are made.In calcium superphosphate series compound fertilizer preparation process, if calcium superphosphate and urea directly mix, and a series of salt-forming reaction can occur, the main component Ca (H in urea and calcium superphosphate
2pO
4)
2h
2there is addition reaction and generate Ca (H in O
2pO
4)
24NH
2cONH
2, release crystal water, batch mixing amount of liquid phase is increased, urea reacts with free phosphoric acid wherein and generates NH simultaneously
2cONH
2h
3pO
4, two kinds of salt all have great solubleness, and easily absorb the moisture in material or in extraneous air, cause material properties severe exacerbation, compound viscosity increases, and presents sposh thick, brings very large difficulty to granulation.Therefore, in calcium superphosphate series compound fertilizer preparation process, conventional methods must carry out neutralizing treatment to calcium superphosphate, a certain amount of alkaline material should be added in advance before adding urea, as magnesium oxide, bicarbonate of ammonia or fused(calcium magnesium)phosphate carry out appropriateness neutralization as neutralizing agent to calcium superphosphate, liquid phase increasing amount after adding with minimizing urea of trying one's best, avoids above-mentioned reaction to occur, and then goes to prepare calcium superphosphate series compound fertilizer.The N-process of calcium superphosphate is complexity, slowly a reaction process, and slight neutralization causes N-process thorough, or excessively neutralization causes again water-soluble phosphorus in calcium superphosphate to become insoluble phosphorus, all to calcium superphosphate quality generation detrimentally affect.
CN1803727A discloses calcium superphosphate production process, this art solutions is for raw material with water, ground phosphate rock and sulfuric acid, first add water and part ground phosphate rock in the reactor, add excess sulfuric acid (being generally 90-95% industrial sulphuric acid) again, add another part ground phosphate rock again and stir, then adding residual sulfuric acid fully react 30-60min in reactor, then mixture being cured, neutralizing agent adjustment free acid content is added again after continuing to stack two weeks, make it≤5.5%.Though the technical scheme that this patent relates to can avoid the waste of phosphate rock resource, reduce production of phosphate fertilizer cost, be particularly useful for applying of medium and small sized enterprises.But the program still consumes large water gaging, and adopt casings in twice method, less economical.CN101913571A discloses a kind of processing method utilizing low-grade phosphate ore stone to produce calcium superphosphate, and the method comprises the steps: P
2o
5after the direct fragmentation of raw ore of≤20%, dry in 80-90 DEG C of tunnel dryer, removing moisture, then carries out abrasive dust operation; After abrasive dust, place 13-15min, then add the dilute sulphuric acid of 70-75% concentration, every 3 parts of weight breezes add 1 part of weight percent sulfuric acid, at 110 DEG C of temperature, stir mixedization; Through changing into, let out, slaking, turn over storehouse and get product.Phosphorus ore available phosphorus transformation efficiency reaches 88%, increases, economizes on resources simultaneously, improve production environment than existing method, reduces production cost.Although the method to utilizing low-grade phosphate ore, improve phosphor resource utilization ratio and have very great help, need to place for some time after phosphorus ore abrasive dust, take up room place; This method is also mixedization using dilute sulphuric acid to carry out acid and ore deposit, and traditional technology is more or less the same.CN102241534A discloses a kind of composite fertilizer and preparation method thereof; the method is that raw material is crushed to the granularity being less than 1mm through pulverizer; then weigh, mix in rear feeding tablets press; add appropriate binding agent and carry out granulation; material after granulation carries out drying, screening, the direct bulk storage of finished product or packaging warehouse-in.The composite fertilizer of preparation includes urea, calcium superphosphate, fused(calcium magnesium)phosphate, Repone K, potassium sulfate, ammonium sulfate.The composite fertilizer utilizing this method to prepare can meet the demand of different levels, also according to crop growth needs, can add Insecticides (tech) & Herbicides (tech) etc. wherein.But this method still depends on the preparation section of traditional Chemical Mixed Fertilizer, the i.e. operation such as raw material pulverizing-mixing-granulation-drying-screening-packaging, though can multielement multifunctional compound fertilizer be obtained, if under the condition that can reach identical fertilizer efficiency, exempt the links such as fertilizer pulverizing, mixing, granulation, screening, be then a kind of technical innovations and breakthroughs, also will bring larger profit space for fertilizer industry.
Summary of the invention
For prior art situation, the object of the invention is to provide one to prepare superphosphate fertilizer, and produces the method for calcium superphosphate series compound fertilizer, simplifies preparation technology, enhances productivity.
For realizing the object of the invention, concentrated acid breeze method of the present invention produces the method for calcium superphosphate and Chemical Mixed Fertilizer thereof, realizes as follows:
A kind of concentrated acid breeze method produces calcium superphosphate method, it is characterized in that, realizes as follows:
First drying, fragmentation, ball mill pulverizing and screening process are carried out to phosphorus ore used, obtained fineness is the ground phosphate rock of 0.15mm-0.20mm, phosphorus ore and sulphuric acid soln is metered in agitation grinding reactor, carry out stirring and grinding, after stirring, grinding 45-60min, placement changes into 150-180min, sends to slaking; Sulfuric acid quality consumption is the 80%-85% of this phosphorus ore theoretical sulfuric acid quality consumption, sulfuric acid mass fraction 82%-87%.
Examination and test of products analysis and control standard is undertaken by GB20413-2006.Water adjusting viscosity can be added in stirring, process of lapping, also in system, directly can add tensio-active agent, carry out with accelerated reaction, improve liquid-solid reaction transformation efficiency, improve the physical property of product.
Further, the invention provides a kind of method that concentrated acid breeze method produces calcium superphosphate series compound fertilizer, it is characterized in that: drying, fragmentation, ball mill pulverizing and screening process are carried out to phosphorus ore used, obtained fineness is the ground phosphate rock of 0.15mm-0.20mm, in agitation grinding reactor, be metered into phosphorus ore and sulphuric acid soln, carry out stirring and grinding 150-180min; Once or in batches add the urea through measuring, Repone K or potassium sulfate, adding magnesium oxide, calcium oxide, bicarbonate of ammonia or fused(calcium magnesium)phosphate is in calcium superphosphate and amendment, after continuing stirring, grinding 60-80min, in granulating equipment after granulation, make composite fertilizer through super-dry, cooling, screening operation; Sulfuric acid quality consumption is the 80%-85% of this phosphorus ore theoretical sulfuric acid quality consumption, sulfuric acid mass fraction 82%-87%.
The mixing process of the present invention by adopting mechanical stirring and abrasive power to act on the vitriol oil and phosphorus ore, by the preparation combination of the preparation of calcium superphosphate, Pre process and Chemical Mixed Fertilizer, directly prepares calcium superphosphate or calcium superphosphate series compound fertilizer.The beneficial effect that the method is brought: under the condition reaching like products standard, the commodity vitriol oil of the industrial 93%-98% mass fraction of direct employing prepares calcium superphosphate, eliminate the sulfuric acid dilution complex acid in calcium superphosphate preparation process or the operation of phosphorus ore wet-milling phosphate ore pulp, eliminate the link such as binder making, raw material pulverizing, Pre process in calcium superphosphate series compound fertilizer material preparation process, simplify preparation technology; Reaction process liquid-solid material macroscopic view big scale stirs and the grinding of microcosmic small scale, enhance the overall and microcosmic local fully mixing effect of sulfuric acid and the liquid-solid material of ground phosphate rock, simultaneously by mechanical abrasive action, weaken or eliminate calcium sulfate wrap film and hinder sulfuric acid and phosphoric acid to problems such as ground phosphate rock internal divergence; Reduce or eliminate the introducing of moisture in system, reduce the corrosive nature of the dilute sulphuric acid in former technique after complex acid to equipment material, reduce the requirement to equipment material, sulfuric acid and phosphorus ore reaction process effect fierceness, the speed of response of subordinate phase is accelerated, reduce calcium superphosphate product water content, improve the physical properties of calcium superphosphate and calcium superphosphate series compound fertilizer product, improve the content of available phosphorus.In a word, this invention simplifies Production Flow Chart, saves and drops into, reduce costs, enhance productivity.For producer's transformation of newly-built calcium superphosphate enterprise and original production calcium superphosphate, it is a kind of positive developing direction.
Embodiment
For illustrating better the present invention, as follows for embodiment:
Embodiment 1
A kind of concentrated acid breeze method produces calcium superphosphate method, it is characterized in that, realizes as follows:
First drying, fragmentation, ball mill pulverizing and screening process are carried out to phosphorus ore used, obtained fineness be 0.15mm-0.20mm(the present embodiment have elect 0.18mm as) ground phosphate rock, phosphorus ore and sulphuric acid soln is metered in agitation grinding reactor, carry out stirring and grinding, 50min is elected in stirring, grinding 45-60min(the present embodiment as) after, placement changes into 150-180min(the present embodiment and elects 160min as), send to slaking; Sulfuric acid quality consumption is that 80%-85%(the present embodiment of this phosphorus ore theoretical sulfuric acid quality consumption elects 83% as), sulfuric acid mass fraction 82%-87%(the present embodiment elects 85% as).
Sampling and measuring its available phosphorus transformation efficiency, moisture and free acid content: available phosphorus transformation efficiency 77.4% mass fraction, free acid 18.2% mass fraction, moisture 4.2% mass fraction.
Embodiment 2
A kind of concentrated acid breeze method produces the method for calcium superphosphate series compound fertilizer, it is characterized in that: drying, fragmentation, ball mill pulverizing and screening process are carried out to phosphorus ore used, obtained fineness be 0.15mm-0.20mm(the present embodiment have elect 0.18mm as) ground phosphate rock, in agitation grinding reactor, be metered into phosphorus ore and sulphuric acid soln, carry out stirring and grind 150-180min(the present embodiment and elect 160min as); Once or in batches add the urea through measuring, Repone K or potassium sulfate, adding magnesium oxide, calcium oxide, bicarbonate of ammonia or fused(calcium magnesium)phosphate is in calcium superphosphate and amendment, continue stirring, grinding 60-80min(the present embodiment elect 70min as) after, in granulating equipment after granulation, make composite fertilizer through super-dry, cooling, screening operation; Sulfuric acid quality consumption is that 80%-85%(the present embodiment of this phosphorus ore theoretical sulfuric acid quality consumption elects 83% as), sulfuric acid mass fraction 82%-87%(the present embodiment elects 85% as).
Then its available phosphorus transformation efficiency, moisture and free acid content of sampling and measuring: available phosphorus transformation efficiency 73.7% mass fraction, free acid 19.3% mass fraction, moisture 6.0% mass fraction.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection domain that all should be included in the claims in the present invention.
Claims (3)
1. produce a calcium superphosphate method, it is characterized in that, realize as follows:
First drying, fragmentation, ball mill pulverizing and screening process are carried out to phosphorus ore used, obtained fineness is the ground phosphate rock of 0.15mm-0.20mm, phosphorus ore and sulphuric acid soln is metered in agitation grinding reactor, carry out stirring and grinding, after stirring, grinding 45-60min, placement changes into 150-180min, sends to slaking; Sulfuric acid quality consumption is the 80%-85% of this phosphorus ore theoretical sulfuric acid quality consumption, sulfuric acid mass fraction 82%-87%.
2. produce the method for calcium superphosphate series compound fertilizer for one kind, it is characterized in that: drying, fragmentation, ball mill pulverizing and screening process are carried out to phosphorus ore used, obtained fineness is the ground phosphate rock of 0.15mm-0.20mm, in agitation grinding reactor, be metered into phosphorus ore and sulphuric acid soln, carry out stirring and grinding 150-180min; Once or in batches add the urea through measuring, Repone K or potassium sulfate, adding magnesium oxide, calcium oxide, bicarbonate of ammonia or fused(calcium magnesium)phosphate is in calcium superphosphate and amendment, after continuing stirring, grinding 60-80min, in granulating equipment after granulation, make composite fertilizer through super-dry, cooling, screening operation; Sulfuric acid quality consumption is the 80%-85% of this phosphorus ore theoretical sulfuric acid quality consumption, sulfuric acid mass fraction 82%-87%.
3. method of producing calcium superphosphate series compound fertilizer as claimed in claim 2, is characterized in that,
Preparing in calcium superphosphate process, according to demand select add phosphorus ammonium, trace element or humic acids, feces of livestock and poultry fertilizer, plant-growth regulator, agricultural chemicals wherein one or more, make composite fertilizer.
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|---|---|---|---|
| CN201510877123.8A CN105254340A (en) | 2015-12-03 | 2015-12-03 | Method for producing calcium superphosphate and calcium superphosphate compound fertilizer |
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|---|---|---|---|
| CN201510877123.8A CN105254340A (en) | 2015-12-03 | 2015-12-03 | Method for producing calcium superphosphate and calcium superphosphate compound fertilizer |
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| CN105254340A true CN105254340A (en) | 2016-01-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673816A (en) * | 2016-12-18 | 2017-05-17 | 贵州越都化工有限公司 | Calcium superphosphate and preparation method thereof |
| CN107244986A (en) * | 2017-08-11 | 2017-10-13 | 句容市白兔镇张峰良品家庭农场 | A kind of vinegrowing matrix and preparation method thereof |
-
2015
- 2015-12-03 CN CN201510877123.8A patent/CN105254340A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673816A (en) * | 2016-12-18 | 2017-05-17 | 贵州越都化工有限公司 | Calcium superphosphate and preparation method thereof |
| CN107244986A (en) * | 2017-08-11 | 2017-10-13 | 句容市白兔镇张峰良品家庭农场 | A kind of vinegrowing matrix and preparation method thereof |
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